CN108398577B - Method for testing reduction degree of graphene oxide - Google Patents
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- CN108398577B CN108398577B CN201810091508.5A CN201810091508A CN108398577B CN 108398577 B CN108398577 B CN 108398577B CN 201810091508 A CN201810091508 A CN 201810091508A CN 108398577 B CN108398577 B CN 108398577B
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Abstract
The invention discloses a method for testing the reduction degree of graphene oxide, which comprises the following steps: s1, determining an electrostatic force microscopic picture of the reduced graphene oxide under different needle point bias voltages by adopting an electrostatic force microscope; s2, plotting the phase of the reduced graphene oxide in the electrostatic force microscopic picture to the tip bias voltage to obtain a phase-tip bias voltage curve; and S3, determining the reduction degree of the reduced graphene oxide compared with the graphene oxide according to the phase-needle tip bias curve. According to the method, by comparing the peak position and the peak intensity change of a phase-needle tip bias curve, the nano-scale representation of the reduction degree difference of the single-layer reduced graphene oxide sample can be carried out after the graphene oxide sample is uniformly reduced by different reduction methods; compared with the prior art, the method can be used as a supplement for methods for characterizing the initial reduction reaction stage, such as an electrostatic force microscope, a scanning polarization force microscope and the like, and is used for enriching characterization ways in the graphene oxide research process.
Description
Technical Field
The invention belongs to the technical field of graphene oxide characterization testing, and particularly relates to a method for testing the reduction degree of graphene oxide.
Background
The characterization and determination of the reduction degree of graphene oxide is an important technology in the field of graphene oxide research.
In the existing technologies for characterizing and testing graphene oxide, the traditional spectroscopy method and the microelectrode-based conductivity testing method can only characterize the occurrence of the reduction reaction of graphene oxide, but the given average information of a test sample is that the reduction reaction of dispersed single-layer graphene oxide cannot be characterized in a nanometer scale; optical observation and a transmission electron microscope can respectively give the color change of the graphene oxide before and after reduction and the change of atomic structure information, but cannot give the difference in performance, so that the reduced graphene oxide lamella with slight difference in reduction degree is difficult to distinguish.
At present, based on the change of the electrical properties of graphene oxide before and after reduction, scanning probe microscopy technologies such as a conductive atomic force microscope, an electrostatic force microscope, a scanning polarization force microscope and the like are used for representing the reduction of the graphene oxide on a nanometer scale, but when the conductive atomic force microscope is used for measurement, the conductive atomic force microscope works in a contact mode, and an electrical loop is formed between a probe and a test sample, so that the electrical induction of reduction or oxidation is easily generated on the test sample, and the reduction degree of the test sample is further influenced; although electrostatic force microscopy and scanning polarization force microscopy can characterize the gradual reduction process of graphene oxide, it is difficult to characterize the difference in the degree of reduction between graphene oxide sheets reduced by different methods when the reduction reaction occurs uniformly across the entire sheet.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for testing the reduction degree of graphene oxide, which is carried out based on an electrostatic force microscope picture and realizes the difference of the reduction degree of the whole reduction-state graphene oxide lamella with uniformly reduced lamella obtained by different reduction methods represented in a nanoscale.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a method for testing the reduction degree of graphene oxide comprises the following steps:
s1, determining an electrostatic force microscopic picture of the reduced graphene oxide under different needle point bias voltages by adopting an electrostatic force microscope;
s2, plotting the phase of the reduced graphene oxide in the electrostatic force microscopic picture to the tip bias voltage to obtain a phase-tip bias voltage curve;
s3, determining the reduction degree of the reduced graphene oxide compared with the graphene oxide according to the phase-needle tip bias curve; in the phase-tip bias curve, the smaller the absolute value of the specific tip bias corresponding to the peak or the valley of the phase and/or the larger the absolute value of the phase under any tip bias smaller than the specific tip bias, the higher the reduction degree of the corresponding reduced graphene oxide compared with the graphene oxide.
Further, in the step S1, the tip bias voltage is in the range of-12V to 12V.
Further, in the step S1, the tip bias interval is 1V.
Further, the reduced graphene oxide is obtained by thermally and/or chemically reducing graphene oxide.
Further, the chemical reduction is that the graphene oxide is placed in saturated hydrazine hydrate steam for reduction.
According to the method, by adopting an electrostatic force microscopic picture method and comparing the peak position and peak intensity change of a phase-needle tip bias voltage curve, nano-scale representation can be carried out on the reduction degree difference of a single-layer reduced graphene oxide sample after the graphene oxide sample is uniformly reduced by different reduction methods; compared with the prior art, the method can be used as a supplement for methods for characterizing the initial reduction reaction stage, such as an electrostatic force microscope, a scanning polarization force microscope and the like, and is used for enriching characterization ways in the graphene oxide research process.
Drawings
The above and other aspects, features and advantages of embodiments of the present invention will become more apparent from the following description taken in conjunction with the accompanying drawings, in which:
fig. 1 is a flowchart of the steps of a method for testing the degree of reduction of graphene oxide according to the present invention;
FIG. 2 is 0 in example 1 according to the present invention#～5#Phase-tip bias curve of the sample;
FIG. 3 is 0 in example 1 according to the present invention#An atomic force microscopy topography of the sample; wherein the white scale represents 1000 nm;
FIG. 4 is 0 in example 1 according to the present invention#Electrostatic force microscopy of the sample at 0V tip bias with respect to FIG. 3 in situ;
FIG. 5 is 0 in example 1 according to the present invention#Electrostatic force microscopy of the sample at 5V tip bias with respect to figure 3 in situ;
FIG. 6 is 0 in example 1 according to the present invention#Electrostatic force microscopy of the sample at-5V from the tip bias in situ of FIG. 3;
FIG. 7 shows example 1 according to the present invention#Electrostatic force micrographs of the sample with tip bias at 5V; wherein the white scale represents 1000 nm;
FIG. 8 shows example 1 according to the present invention#Electrostatic force microscopy of the sample at-5V tip bias with respect to FIG. 7 in situ;
FIG. 9 shows example 2 of embodiment 1 according to the present invention#Electrostatic force micrographs of the sample with tip bias at 5V; wherein the white scale represents 1000 nm;
FIG. 10 shows example 2 of embodiment 1 according to the present invention#Electrostatic force microscopy of the sample at-5V with the tip biased in situ in FIG. 9;
FIG. 11 shows example 3 of embodiment 1 according to the present invention#Electrostatic force micrographs of the sample with tip bias at 5V; wherein the white scale represents 1000 nm;
FIG. 12 shows example 3 of embodiment 1 according to the present invention#Electrostatic force microscopy of the sample at-5V tip bias with respect to FIG. 11 in situ;
FIG. 13 shows example 4 of embodiment 1 according to the present invention#Electrostatic force micrographs of the sample with tip bias at 5V; wherein the white scale represents 1000 nm;
FIG. 14 shows example 4 of embodiment 1 according to the present invention#Sample and static at-5V tip bias in situ in FIG. 13An electric power microscope picture;
FIG. 15 shows example 5 of embodiment 1 according to the present invention#Electrostatic force micrographs of the sample with tip bias at 5V; wherein the white scale represents 1000 nm;
FIG. 16 shows example 5 of embodiment 1 according to the present invention#Electrostatic force microscopy of the sample at-5V tip bias with respect to FIG. 15 in situ;
FIG. 17 is 0 in comparative example 1 according to the present invention#Samples and 5#Analyzing an X-ray photoelectron spectroscopy test spectrogram of the sample;
FIG. 18 is 0 in comparative example 1 according to the present invention#～5#An X-ray photoelectron spectroscopy test spectrogram of the sample;
FIG. 19 is 0 in comparative example 2 according to the present invention#～5#A normalized ultraviolet visible absorption spectrum of the sample;
FIG. 20 is 0 in comparative example 3 according to the present invention#A scanning polarization force micrograph of the sample;
FIG. 21 is 0 in situ with FIG. 20 in comparative example 3 according to the present invention#Scanning polarization force microscope picture of sample reduced at 150 deg.C for 15 min;
FIG. 22 is 0 in situ with FIG. 20 in comparative example 3 according to the present invention#Scanning polarization force microscope picture of sample after reducing 75min at 150 ℃;
FIG. 23 is comparative example No. 3 1 according to the present invention#A scanning polarization force micrograph of the sample; wherein, the white square frame is in-situ 1#An atomic force microscopy topography of the sample; white scale indicates 1000 nm;
FIG. 24 is 0 in comparative example 3 according to the present invention#Samples and 5#An atomic force microscopy topography of a mixture of samples; wherein the white scale represents 1000 nm;
FIG. 25 is 0 in situ with FIG. 24 in comparative example 3 according to the present invention#Samples and 5#A scanning polarization force micrograph of a mixture of samples;
FIG. 26 is comparative example 3, 5, according to the present invention#An atomic force microscopy topography of the sample; wherein the white scaleRepresents 1000 nm;
FIG. 27 is 5 in situ with FIG. 26 in comparative example 3 according to the present invention#Scanning polarization force microscopy of samples.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the specific embodiments set forth herein. Rather, these embodiments are provided to explain the principles of the invention and its practical application to thereby enable others skilled in the art to understand the invention for various embodiments and with various modifications as are suited to the particular use contemplated.
The invention discloses a method for testing the reduction degree of graphene oxide, which comprises the following steps of:
in step S1, electrostatic force micrographs of the reduced graphene oxide at different tip biases were determined using an electrostatic force microscope.
Specifically, reduced graphene oxide is obtained by thermally and/or chemically reducing graphene oxide; the chemical reduction is preferably carried out by placing graphene oxide in saturated hydrazine hydrate steam for reduction.
The test range of the needle tip bias voltage of the graphene oxide is-12V, and the interval is preferably 1V.
In step S2, the phase of the reduced graphene oxide in the electrostatic force microscopy is plotted against the tip bias voltage to obtain a phase-tip bias voltage curve.
In step S3, the degree of reduction of the reduced graphene oxide compared to the graphene oxide is determined according to the phase-tip bias curve.
Specifically, in the phase-tip bias curve, the smaller the absolute value of the specific tip bias corresponding to the peak or the valley of the phase, and/or the larger the absolute value of the phase at any tip bias smaller than the specific tip bias, the higher the reduction degree of the corresponding reduced graphene oxide compared to the graphene oxide.
Thus, according to the determination method of the present invention, the reduction degree of different reduced graphene oxides compared to that of graphene oxide can be compared.
To illustrate the beneficial effects of the above test methods, different samples were obtained by performing different modes of reduction with graphene oxide and determined accordingly, as described in example 1 below.
Example 1
Specifically, the samples were prepared using the following method: firstly, 10 mu L of Graphene Oxide (GO) suspension liquid with the concentration of 0.5mg/mL is dripped on the surface of newly-cleaved mica, and is dried by an ear washing ball after being adsorbed for 30s to obtain a GO sample; then, reducing the GO sample by adopting different methods to respectively obtain reduced graphene oxide (rGO) samples.
More specifically, the above GO samples were reduced with reference to the method in table 1 below.
TABLE 1 sample numbering and conditions of acquisition
In the range of-12V to 12V needle tip bias, 1V interval is adopted for 0#～5#The sample is measured by an electrostatic force microscope; in each of the obtained electrostatic force micrographs, a phase value is generated.
Thus, each sample correspondingly generates 25 phase values, the phase values are taken as vertical coordinates, and the corresponding needle point bias voltage is taken as horizontal coordinates to make a phase-needle point bias voltage curve; as shown in fig. 2.
Determining the peak or valley value of each sample and the corresponding tip bias voltage according to the six phase-tip bias curves in fig. 2; as shown in table 2.
As can be seen from FIG. 2, 0#The phase of the sample is positive, and 1#～5#The phase of the sample is negative, which indicates that the phase is from 0#Sample No. 1#～5#The sample is subjected to reduction reaction; and from 1#Sample Change to 5#In the sample, the phase contrast is significantly enhanced, as shown in fig. 2 at the dashed line. As can be seen from the combination of Table 2, 1#～5#In the sample, the absolute values of the specific needle tip bias voltages corresponding to the valleys are reduced in sequence, which indicates that the reduction degree of the sample is 1#Sample No. 5#The order of the samples deepens, as indicated by the transverse arrows in FIG. 2; and is in 1#～5#In the sample, the absolute values of the phases corresponding to any tip biases smaller than the above-mentioned specific tip bias (tip bias corresponding to the peak or valley) were sequentially increased, which also indicates that the reduction degree of the sample was 1#Sample No. 5#The order of the samples deepens as indicated by the longitudinal arrows in fig. 2. It follows that, in the present embodiment, 0#～5#The reduction degree of the sample is from shallow to deep in the order: 0#Sample < 1#Sample ≈ 2#Sample < 3#Sample ≈ 4#Sample < 5#And (3) sampling.
That is to say, in the test method of this embodiment, according to the phase-tip bias diagram, the smaller the absolute value of the specific tip bias corresponding to the peak or the valley of the phase, and/or the larger the absolute value of the phase under any tip bias smaller than the specific tip bias, the higher the reduction degree of the corresponding reduced graphene oxide compared to the graphene oxide.
In addition, as can be seen from fig. 2, the phase contrast is significantly enhanced at the dotted lines, and thus 0 is shown respectively#～5#Electrostatic Force micrographs of samples under tip bias of-5V and 5V, respectively, and to compare the in situ measurements, an Atomic Force Microscope (AFM) was first used for 0#The sample was characterized as shown in fig. 3; to show that the elevation mode of electrostatic force microscopy imaging has been removedInfluence of appearance information, electrostatic force microscope pair 0 under 0V needle tip bias#The sample was characterized in situ with respect to fig. 3, as shown in fig. 4, without any effect of topographical information throughout the plot; 0#～5#The electrostatic force micrographs of the samples under tip bias of-5V and 5V, respectively, are shown in fig. 5-16, respectively, and the corresponding phases are apparent from fig. 5-16.
To further verify the beneficial effects of the test method shown in example 1 above, other characterization means were used for the above 0#～5#The samples were characterized as shown in comparative examples 1-3 below.
Comparative example 1
In the present comparative example, 0 was characterized by X-ray photoelectron spectroscopy (XPS)#～5#And (3) sampling.
FIG. 17 shows 0#Samples and 5#The analytical X-ray photoelectron spectroscopy test spectrum of the sample, i.e., the deconvolution obtained peaks (denoted by a, C, b, and d, respectively) with binding energies of 284.5eV, 285.5eV, 286.9eV, and 288.5eV, which represent C ═ C/C (aromatic ring), C — O (epoxy group and alkoxy group), C ═ O, and COOH group, respectively. As can be seen from FIG. 17, after the sample reduction (5)#Sample) has a significant reduction in carbon atoms bound to oxygen, indicating that a significant portion of the oxygen-containing functional groups have been removed; and from the XPS data, it can be concluded that for the sample after chemical reduction (5)#Sample), the ratio of carbon atoms in the aromatic ring to the oxygen-containing functional group increased from the initial 1.1:1 to 6.3: 1.
FIG. 18 shows 0#～5#XPS spectra of the samples, it is clear that 1 for various degrees of reduction#～5#Differences between samples are difficult to see from nearly overlapping XPS spectra; that is, the XPS test method in this comparative example cannot distinguish between reduced graphene oxides of different degrees of reduction as in example 1 above.
Comparative example 2
In this comparative example, 0 is respectively characterized by UV-visible absorption#～5#And (3) sampling.
FIG. 19 shows 0#～5#And (3) a spectrum of the normalized ultraviolet-visible absorption spectrum of the sample. As can be seen from FIG. 19, relative to 0#Sample, 1#～5#The major absorption peak of the sample was red-shifted from 226nm to around 264nm, the absorption in the visible region was enhanced, and the shoulder of the peak around 300nm disappeared, all indicating the removal of the oxygen-containing functional group and the repair of the pi-conjugated structure in the graphene nanosheet layer. However, except for the high temperature (450 ℃ C.) in air and the oxidation couple 2#Apparent breakdown of light transmission by the sample, 1#～5#The samples did not differ otherwise.
Therefore, the test means of uv-vis absorption in this comparative example cannot distinguish between reduced graphene oxides of different degrees of reduction as in example 1 above.
Comparative example 3
In the present comparative example, 0 was characterized by using a Scanning Polarization Force Microscope (SPFM), respectively#～5#And (3) sampling.
Figures 20 to 27 show SPFM plots for different samples respectively. It is worth noting that in SPFM plots, an increase in apparent height compared to actual topography height can indicate reduction of GO samples.
As can be seen from the figures, the reduction reaction occurs uniformly (FIGS. 22, 23, 25) or non-uniformly (positions indicated by the longitudinal arrows in FIGS. 21, 27); it is clear that when the GO sheets are uniformly reduced by different methods, 1#～5#The difference in reduction degree between the respective samples is difficult to see by comparison of the apparent heights, because the SPFM map includes topographic information (positions indicated by lateral arrows in fig. 25, 27), and the SPFM imaging is susceptible to the set magnitude of the imaging force (set value). That is, the SPFM test method in this comparative example cannot distinguish the reduced graphene oxide having different reduction degrees and uniformly occurring reduction reaction as in example 1.
In summary, according to the method for testing the reduction degree of graphene oxide of the present invention, compared with the prior art, after a graphene oxide sample is uniformly reduced by different reduction methods, the difference in the reduction degree of a single-layer reduced graphene oxide sample can be characterized in a nanometer scale by comparing the peak position and the peak intensity change of a phase-tip bias curve by using an electrostatic force microscopy method.
While the invention has been shown and described with reference to certain embodiments, those skilled in the art will understand that: various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (10)
1. A method for testing the reduction degree of graphene oxide is characterized by comprising the following steps:
s0-1, determining a first electrostatic force microscopic picture of the graphene oxide under different needle tip bias voltages by using an electrostatic force microscope;
s0-2, plotting the phase of the graphene oxide to the tip bias voltage in the first electrostatic force microscopic picture to obtain a first phase-tip bias voltage curve;
s1, determining an electrostatic force microscopic picture of the reduced graphene oxide under different needle point bias voltages by adopting an electrostatic force microscope;
s2, plotting the phase of the reduced graphene oxide in the electrostatic force microscopic picture to the tip bias voltage to obtain a phase-tip bias voltage curve;
s3, determining the reduction degree of the reduced graphene oxide compared with the graphene oxide according to the first phase-needle tip bias curve and the phase-needle tip bias curve; in the first phase-needle tip bias curve and the phase-needle tip bias curve, the smaller the absolute value of a specific needle tip bias corresponding to the peak or valley of the phase, and/or the larger the absolute value of the phase under any needle tip bias smaller than the specific needle tip bias, the higher the reduction degree of the corresponding reduced graphene oxide compared with the graphene oxide.
2. The test method of claim 1, wherein in the step S1, the tip bias voltage is in the range of-12V to 12V.
3. The test method of claim 2, wherein in step S1, the tip bias interval is 1V.
4. The test method according to any one of claims 1 to 3, wherein the reduced graphene oxide is obtained by thermally and/or chemically reducing graphene oxide.
5. The test method according to claim 4, wherein the chemical reduction is a reduction of the graphene oxide in saturated hydrazine hydrate vapor.
6. A method for testing the reduction degree of graphene oxide is characterized by comprising the following steps:
s1, measuring electrostatic force microscopic pictures of at least two reduced graphene oxides under different needle point bias voltages by adopting an electrostatic force microscope; each of the at least two reduced graphene oxides receives a different reduction process;
s2, respectively plotting the phases of the at least two reduced graphene oxides in the electrostatic force microscopic picture to the tip bias voltage to obtain at least two phase-tip bias voltage curves;
s3, determining the reduction degree of the at least two reduced graphene oxides according to the phase-needle tip bias curve; in the phase-tip bias curve, there is a valley of the phase, and the smaller the absolute value of the specific tip bias corresponding to the valley of the phase is, and/or the larger the absolute value of the phase under any tip bias smaller than the specific tip bias is, the higher the reduction degree of the corresponding reduced graphene oxide is.
7. The test method of claim 6, wherein in the step S1, the tip bias voltage is in the range of-12V to 12V.
8. The test method of claim 7, wherein in step S1, the tip bias interval is 1V.
9. The test method according to any one of claims 6 to 8, wherein the reduced graphene oxide is obtained by thermally and/or chemically reducing graphene oxide.
10. The test method according to claim 9, wherein the chemical reduction is a reduction of the graphene oxide in saturated hydrazine hydrate vapor.
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